WO2022188550A1 - Main and auxiliary alloy-based neodymium-iron-boron magnet material and preparation method therefor - Google Patents
Main and auxiliary alloy-based neodymium-iron-boron magnet material and preparation method therefor Download PDFInfo
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- WO2022188550A1 WO2022188550A1 PCT/CN2022/072244 CN2022072244W WO2022188550A1 WO 2022188550 A1 WO2022188550 A1 WO 2022188550A1 CN 2022072244 W CN2022072244 W CN 2022072244W WO 2022188550 A1 WO2022188550 A1 WO 2022188550A1
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 280
- 239000000956 alloy Substances 0.000 title claims abstract description 280
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 66
- 239000000463 material Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 232
- 239000000203 mixture Substances 0.000 claims abstract description 41
- 229910052779 Neodymium Inorganic materials 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 23
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 19
- 229910052733 gallium Inorganic materials 0.000 claims description 18
- 229910052802 copper Inorganic materials 0.000 claims description 16
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 13
- 230000005291 magnetic effect Effects 0.000 claims description 12
- AADMRFXTAGXWSE-UHFFFAOYSA-N monoacetoxyscirpenol Natural products CC(=O)OC1C(O)C2OC3(C)C=C(C)CCC3(CO)C1(C)C24CO4 AADMRFXTAGXWSE-UHFFFAOYSA-N 0.000 claims description 10
- 150000002910 rare earth metals Chemical class 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- 229910052726 zirconium Inorganic materials 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 9
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 229910052689 Holmium Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
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- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 238000003723 Smelting Methods 0.000 claims description 5
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 229910052735 hafnium Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 238000009749 continuous casting Methods 0.000 claims description 3
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 3
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- 239000011258 core-shell material Substances 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
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- 230000008569 process Effects 0.000 description 9
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- 239000010410 layer Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
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- 230000005347 demagnetization Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005292 diamagnetic effect Effects 0.000 description 2
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
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- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0572—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
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- C22C33/00—Making ferrous alloys
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- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
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- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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Definitions
- NdFeB has attracted much attention as the permanent magnet with the largest magnetic energy product at room temperature, and is widely used in traction motors, servo motors, main drive motors of new energy vehicles, magnetic components, wind turbines and other fields.
- the demagnetization resistance of commercial magnets is only 1/4 of the theoretical value (about 71KOe).
- the anti-demagnetization ability of NdFeB is generally characterized by coercive force, which is greatly affected by the microstructure of NdFeB, and is controlled by two mechanisms, nucleation field and pinning field, dominated by nucleation field. , the way of nucleation field to improve HcJ is to eliminate the reverse domain nucleation point. From a microscopic point of view, there are generally three ways to improve coercivity:
- the specific method is to absorb Fe in the grain boundary through the main phase containing Nd 6 Fe 13 X, so that the grain boundary phase is transformed into a non-magnetic phase or an antiferromagnetic phase. , at the same time widen the grain boundary; or increase the total rare earth content to increase the volume of the grain boundary phase; through the addition of grain boundary elements such as Cu, Ga, Co, Al, etc., improve the fluidity of the neodymium-rich phase and optimize the grain boundary of the main phase, thereby Repair the main phase defects, reduce the formation of reverse domains, and improve HcJ.
- the HcJ that such methods can improve is limited, and it is difficult to increase HcJ above 25kOe.
- the anisotropy field of the main phase is improved by the addition of heavy rare earths, while the reserves of heavy rare earth resources are small and the price is high, which seriously restricts the application of NdFeB magnets in various industries.
- the heavy rare earth is distributed along the layer outside the main phase by means of double alloying or diffusion, so as to improve the utilization rate of heavy rare earth.
- the diffusion method cannot be applied to magnets with larger thickness (>15 mm), and the existing double alloy method has limited improvement effect (about 1-1.5 kOe can increase HcJ).
- the invention provides a raw material composition of a main and auxiliary alloy system NdFeB magnet material, which includes a main alloy raw material and an auxiliary alloy raw material; wherein, the main alloy raw material includes the following components: light rare earth element LR, 10.0-33.0 mas%; LR is selected from one or more of Y, La, Ce, Pr, Nd; heavy rare earth element HR, 0-20.0 mas%; HR is selected from one or more of Gd, Dy, Tb and Ho M, 0.1 ⁇ 5.0mas%; M is selected from one or more of Co, Cu, Al and Ga; X, 0.05 ⁇ 0.7mas%; X is selected from one or more of Zr, Ti and Nb ; B, 0.94-1.1 mas%; the balance is Fe; wherein, mas% refers to the mass percentage of the components in the main alloy raw material;
- the auxiliary alloy raw material includes the following components: light rare earth element LR, 0-30.0 mas%; LR is Nd and/or Pr; heavy rare earth element HR, 1-80 mas%; HR is Dy and/or Tb; M, 5.0 ⁇ 20.0mas%; M is selected from one or more of Co, Cu, Al and Ga; X, 3.0 ⁇ 12.0mas%; X is selected from one or more of Ti, Zr, Hf, Nb, W and Ta Various; B, 0-0.6 mas%; the balance is Fe; wherein, mas% refers to the mass percentage of the components in the auxiliary alloy raw material;
- the mass percentage of the auxiliary alloy raw material in the raw material composition of the main and auxiliary alloy-based NdFeB magnet material is 1.0-15.0 mas%.
- the content of the LR is preferably 25.0-30.0 mas%, such as 25.2 mas%, 29.5 mas% or 30 mas%, mas% refers to the composition in the main alloy raw material. mass percentage in .
- the content of the Pr is preferably 6.0-7.5 mas%, for example, 6.3 mas% or 7.375 mas%.
- the mass percentage in the main alloy raw material is preferably 6.0-7.5 mas%, for example, 6.3 mas% or 7.375 mas%.
- the LR contains Nd and Pr. More preferably, the Nd content is 22.125 mas %, and the Pr content is 7.375 mas %; or, the Nd content is 22.5 mas %, and the Pr content is 7.5 mas %; or, the The content of Nd is 18.9 mas%, and the content of Pr is 6.3 mas%; mas% refers to the mass percentage of components in the main alloy raw material.
- the content of the HR is preferably 1.0-10.0 mas%, such as 1.5 mas% or 5.3 mas%, and mas% refers to the mass of the components in the main alloy raw material percentage.
- the content of Dy is preferably 1.0-5.0 mas%, for example, 1.5 mas% or 4.3 mas%.
- the HR is Dy; the content of Dy is preferably 1.5 mas%.
- mas% refers to the mass percentage of components in the main alloy raw material.
- the content of M is preferably 0.5-2.0 mas%, such as 0.88 mas%, 1.5 mas% or 1.65 mas%, mas% refers to the composition in the main alloy The mass percentage of the raw material.
- the content of Ga is preferably 0.2-0.4 mas%, such as 0.25 mas%, mas% refers to the composition in the main alloy The mass percentage of the raw material.
- the content of the Al is preferably 0.01-0.1 mas%, such as 0.03 mas%, mas% refers to the composition in the main alloy The mass percentage of the raw material.
- the content of Cu is preferably 0.1-0.25 mas%, for example, 0.15 mas%, mas% refers to the composition in the main alloy The mass percentage of the raw material.
- the content of Co is preferably 0.5-1.0 mas%, and mas% refers to the mass percentage of the component in the main alloy raw material .
- the M includes Ga, Al, Cu and Co; wherein, the content of the Ga is preferably 0.25mas%, and the content of the Al is preferably 0.03mas% , the content of the Cu is preferably 0.1 mas%, and the content of the Co is preferably 0.5 mas%.
- mas% refers to the mass percentage of components in the main alloy raw material.
- the content of X is preferably 0.1-0.35 mas%, for example, 0.11 mas% or 0.15 mas%, and mas% refers to the mass of the components in the main alloy raw material percentage.
- the X is Zr or Ti.
- the content of B is preferably 0.97-0.99 mas%, such as 0.98 mas%, where mas% refers to the mass percentage of the component in the main alloy raw material.
- the main alloy raw material includes the following components: Nd, 22.125mas%; Pr, 7.375mas%; Ga, 0.25mas%; Al, 0.03mas%; Cu, 0.1mas%; Co , 0.5mas%; Zr, 0.11mas%; B, 0.98mas%; the balance is Fe; wherein, mas% refers to the mass percentage of components in the main alloy raw material.
- the main alloy raw material includes the following components: Nd, 22.5mas%; Pr, 7.5mas%; Dy, 1.5mas%; Ga, 0.4mas%; Cu, 0.25mas%; Co , 1.0mas%; Zr, 0.35mas%; B, 0.97mas%; the balance is Fe; wherein, mas% refers to the mass percentage of components in the main alloy raw material.
- the main alloy raw material includes the following components: Nd, 18.9mas%; Pr, 6.3mas%; Dy, 4.3mas%; Ho, 1.0mas%; Ga, 0.25mas%; Al , 0.1mas%; Cu, 0.15mas%; Co, 1.0mas%; Ti, 0.15mas%; B, 0.97mas%; mass percentage.
- the total rare earth content TRE in the auxiliary alloy raw material is preferably 35.0-50.0 mas%, more preferably 40.0-45.0 mas%, and mas% refers to the mass percentage of the components in the auxiliary alloy raw material .
- the content of the LR is preferably 20.0-30.0 mas%, such as 25.0 mas%, and mas% refers to the mass percentage of the components in the auxiliary alloy raw material.
- the content of the Nd is preferably 10.0-20.0 mas%, such as 15.0 mas%, mas% refers to the component in the auxiliary alloy The mass percentage of the raw material.
- the content of the Pr is preferably 15.0-25.0 mas%, for example, 20.0 mas%, and mas% refers to the components in the auxiliary alloy.
- the mass percentage of the raw material is preferably 15.0-25.0 mas%, for example, 20.0 mas%, and mas% refers to the components in the auxiliary alloy.
- the LR is Nd and Pr, the content of Nd is 15.0 mas%, and the content of Pr is 15.0 mas%; mas% refers to the components in the auxiliary alloy.
- the mass percentage of the raw material is Nd and Pr, the content of Nd is 15.0 mas%, and the content of Pr is 15.0 mas%; mas% refers to the components in the auxiliary alloy. The mass percentage of the raw material.
- the content of the HR is preferably 15.0-20.0 mas%, and mas% refers to the mass percentage of the components in the auxiliary alloy raw material.
- the HR is Tb
- the content of Tb is 15.0 mas%
- mas% refers to the mass percentage of the components in the auxiliary alloy raw material.
- the HR is Dy
- the content of Dy is 20.0 mas%
- mas% refers to the mass percentage of the components in the auxiliary alloy raw material.
- the content of the Ga is preferably 2.0-10.0 mas%, for example, 5.0 mas%, mas% refers to the composition in the auxiliary alloy The mass percentage of the raw material.
- the content of Co is preferably 10.0-20.0 mas%, such as 15.0 mas%, mas% refers to the composition in the auxiliary alloy The mass percentage of the raw material.
- the M is Ga and Co; wherein, the content of the Ga is preferably 5.0mas%, the content of the Co is preferably 15.0mas%, and the mas% is Refers to the mass percentage of the components in the auxiliary alloy raw material.
- the content of X is preferably 4.0-10.0 mas%, such as 4.5 mas% or 5.0 mas%, and mas% refers to the quality of the components in the auxiliary alloy raw material percentage.
- the X is Zr.
- the auxiliary alloy raw material includes the following components: Pr, 25.0mas%; Dy, 20.0mas%; Zr, 4.5mas%; B, 0.5mas%; the balance is Fe; wherein, mas% refers to the mass percentage of components in the auxiliary alloy raw material.
- the mass percentage of the auxiliary alloy raw material in the raw material composition of the main and auxiliary alloy NdFeB magnet material is preferably 2.0-5.0 mas%, for example, 4.0 mas%.
- the main and auxiliary alloys are raw material compositions of NdFeB magnet materials, which include main alloy raw materials and auxiliary alloy raw materials; wherein, the main alloy raw materials include the following components: Nd, 22.125 mas%; Pr, 7.375mas%; Ga, 0.25mas%; Al, 0.03mas%; Cu, 0.1mas%; Co, 0.5mas%; Zr, 0.11mas%; B, 0.98mas%; the balance is Fe; Wherein, mas% refers to the mass percentage of components in the main alloy raw material; the auxiliary alloy raw material includes the following components: Nd, 15.0mas%; Pr, 15.0mas%; Tb, 15.0mas%; Zr, 10.0 mas%; B, 0.5mas%; the balance is Fe; wherein, mas% refers to the mass percentage of the components in the auxiliary alloy raw materials; the auxiliary alloy raw materials are in the main and auxiliary alloy NdFeB magnet materials The mass percentage in the raw material composition is 4.0 mas%.
- the main and auxiliary alloy is a raw material composition of NdFeB magnet material, which includes a main alloy raw material and an auxiliary alloy raw material; wherein, the main alloy raw material includes the following components: Nd, 22.5 mas%; Pr, 7.5mas%; Dy, 1.5mas%; Ga, 0.4mas%; Cu, 0.25mas%; Co, 1.0mas%; Zr, 0.35mas%; B, 0.97mas%; the balance is Fe; Wherein, mas% refers to the mass percentage of components in the main alloy raw material; the auxiliary alloy raw material includes the following components: Pr, 25.0mas%; Dy, 20.0mas%; Zr, 4.5mas%; B, 0.5 mas%; the balance is Fe; wherein, mas% refers to the mass percentage of the components in the auxiliary alloy raw materials; the proportion of the auxiliary alloy raw materials in the raw material composition of the main and auxiliary alloy NdFeB magnet materials The mass percentage is 5.0mas%.
- the present invention also provides a preparation method of a main and auxiliary alloy system NdFeB magnet material, which comprises the following steps:
- the main alloy and the auxiliary alloy are hydrogen crushed and finely pulverized, respectively, and then mixed, and subjected to forming and sintering treatment to obtain the main and auxiliary alloy NdFeB magnet material.
- the melting, the casting, the hydrogen crushing, the micro-pulverization, the molding, and the sintering are all conventional operation modes and conditions in the art.
- the melting can be performed according to conventional melting in the art, for example, melting in a melting furnace.
- the vacuum degree of the melting furnace is about 5 ⁇ 10 -2 Pa.
- the melting temperature may be 1300°C to 1600°C, preferably 1500°C to 1550°C.
- the casting process can be a conventional casting process in the field, such as a thin strip continuous casting method, an ingot casting method, a centrifugal casting method or a rapid quenching method.
- the process of the hydrogen fragmentation can be a conventional process in the art.
- the dehydrogenation temperature of the hydrogen fragmentation may be 400-650°C, for example, 500-620°C.
- the micro-pulverization process can be a conventional micro-pulverization process in the art.
- the pulverization is preferably carried out in a jet mill.
- the micro-pulverization is preferably performed in an oxygen-containing atmosphere; the oxygen content in the oxygen-containing atmosphere may be below 80 ppm, preferably below 50 ppm.
- the particle size of the finely pulverized powder may be 1-20 ⁇ m.
- the forming conditions can be conventional in the field, such as pressing in a press to form a green body.
- the magnetic field strength of the press is preferably 0.5T-3.0T, such as 1.0-2.0T.
- the pressing pressure may be 200 ⁇ 300 MPa, for example, 260 MPa.
- the pressing time may be conventional in the art, and may be 3-30s, for example, 15s.
- the sintering conditions may be conventional in the field.
- the sintering temperature may be 1000-1150°C, preferably 1060-1090°C.
- the sintering time may be 4-20 hours.
- the sintering atmosphere is preferably vacuum or argon atmosphere.
- the present invention also provides a main and auxiliary alloy system NdFeB magnet material, which is prepared according to the preparation method of the main and auxiliary alloy system NdFeB magnet material.
- the main and auxiliary alloy NdFeB magnet material includes a main phase and a grain boundary phase; wherein, the main phase is a core-shell structure, the core is LR 2 T 14 B, and the shell is HR 2 T 14 B; the grain boundary phase includes neodymium-rich phase, XB 2 phase and R 6 T 13 M phase;
- R is LR and/or HR
- LR is selected from one or more of Y, La, Ce, Pr, Nd;
- HR is selected from one or more of Gd, Dy, Tb and Ho;
- M is selected from one or more of Cu, Al and Ga;
- X is selected from one or more of Ti, Zr, Hf, Nb, W and Ta;
- T Fe and/or Co.
- LR is Pr and Nd; HR is Tb; M is Cu, Al and Ga; X is Zr; T is Fe and Co.
- LR is Pr and Nd; HR is Dy; M is Cu and Ga; X is Zr; and T is Fe and Co.
- LR is Pr and Nd; HR is Dy and Ho; M is Cu, Al and Ga; X is Ti; T is Fe and Co.
- the main alloy provides LR 2 Fe 14 B main phase and a certain neodymium-rich phase
- the auxiliary alloy provides HR as a diffusion source.
- the HR in the auxiliary alloy passes through the molten neodymium-rich phase.
- the surface layer of the main phase particles diffuses and replaces the LR of the main phase particles, thereby forming a heavy rare earth shell HR 2 Fe 14 B on the surface layer of the main phase.
- the low content of B in the auxiliary alloy exists in the form of solid solution, reducing the existence of HR 2 T 14 B, making it easier for HR to form a shell layer on the outer edge of the main phase particles during the mixing process, thereby improving the utilization efficiency of HR; at the same time,
- the low content of B makes the auxiliary alloy flakes more easily broken, which is convenient for the normal operation of the smelting equipment and for the next hydrogen crushing.
- the X element in the neodymium-rich phase combines with B to form a precipitate XB 2 at high temperature, and the original R-Fe-X and Fe in the Fe-X are released, Thereby, the fluidity of the neodymium-rich phase is improved, and the formation of R 6 T 13 M phase (tetragonal phase, non-magnetic phase or diamagnetic phase) is promoted by M elements, etc., thereby ensuring high remanence (Br) and improving the internal magnetism of the magnet. Intrinsic coercivity (HcJ).
- the present invention forms a shell layer of heavy rare earth on the NdFeB main phase particles by constructing the main and auxiliary alloy matching methods, combined with a specific raw material ratio, and at the same time improves the fluidity of the Nd-rich phase, so as to ensure high remanence at the same time.
- the intrinsic coercivity of the magnet is improved.
- the preparation method of the invention is simple and feasible, and can be applied in engineering.
- FIG. 1 is a TEM image of the main and auxiliary alloy-based NdFeB magnet material in Example 3 of the present invention.
- Example 2 is an elemental analysis diagram of the main and auxiliary alloy-based NdFeB magnet material in Example 1 of the present invention.
- step (1) Hydrogen crushing process: at room temperature, the main alloy flakes and the auxiliary alloy flakes in step (1) are respectively subjected to hydrogen absorption, and then subjected to vacuum dehydrogenation treatment at 500-620° C. to obtain coarsely pulverized powder.
- Micro-pulverization treatment The coarsely pulverized powder in step (2) is pulverized in an atmosphere with an oxygen content of 50 ppm or less in a jet mill to obtain a finely pulverized powder with an average particle size of 1-20 ⁇ m.
- Forming process press in a press with a magnetic field strength of 1.0 to 2.0T to form a green body, and then hold it for 15 s under the condition of a pressure of 260 MPa to obtain a formed body.
- the formed body is sintered at a temperature of 1060-1090°C, and the sintering atmosphere is a vacuum or an argon atmosphere to obtain a NdFeB permanent magnet material.
- FIG. 1 shows the element distribution of the Ti-rich region in the grain boundary phase. It can be seen that Ti and B elements are closely related. Combining the phase diagram and thermodynamic calculations, it can be known that this phase is TiB 2 , while Zr, Ti, Hf and other elements are of the same family. This phase can be produced in the production of boron.
- TiB 2 is a high-temperature ceramic phase, which is stable in a large temperature region, thereby purifying B in the grain boundary, making the neodymium-rich phase more fluid, and providing favorable conditions for the formation of tetragonal Nd 6 Fe 13 Ga and other phases. condition.
- the main and auxiliary alloy NdFeB magnet materials prepared in Examples 1 to 3 were taken, and the magnetic properties were detected by using the PFM14.CN type ultra-high coercivity permanent magnet measuring instrument of China Metrology Institute.
- Example 2 Br(kGs) 14.3 13.1 12.2 HcJ(kOe) 18.9 24.5 30.5
- Br refers to remanence; after the permanent magnet material is saturated magnetized, the magnetism that can be maintained by the external magnetic field is removed, which is called remanence. Magnetic polarization coercivity H cJ (intrinsic coercivity).
Abstract
Description
编号Numbering | 实施例1Example 1 | 实施例2Example 2 | 实施例3Example 3 |
Br(kGs)Br(kGs) | 14.314.3 | 13.113.1 | 12.212.2 |
HcJ(kOe)HcJ(kOe) | 18.918.9 | 24.524.5 | 30.530.5 |
Claims (10)
- 一种主辅合金系钕铁硼磁体材料的原料组合物,其包括主合金原料和辅合金原料;其中,所述主合金原料包括以下组分:轻稀土元素LR,10.0~33.0mas%;LR选自Y、La、Ce、Pr、Nd的一种或多种;重稀土元素HR,0~20.0mas%;HR选自Gd、Dy、Tb和Ho中的一种或多种;M,0.1~5.0mas%;M选自Co、Cu、Al和Ga中的一种或多种;X,0.05~0.7mas%;X选自Zr、Ti和Nb中的一种或多种;B,0.94~1.1mas%;余量为Fe;其中,mas%是指组分在所述主合金原料中的质量百分比;A raw material composition of a main and auxiliary alloy system NdFeB magnet material, which includes a main alloy raw material and an auxiliary alloy raw material; wherein, the main alloy raw material includes the following components: light rare earth element LR, 10.0-33.0 mas%; LR One or more selected from Y, La, Ce, Pr, Nd; heavy rare earth element HR, 0-20.0 mas%; HR selected from one or more of Gd, Dy, Tb and Ho; M, 0.1 ~5.0mas%; M is selected from one or more of Co, Cu, Al and Ga; X, 0.05~0.7mas%; X is selected from one or more of Zr, Ti and Nb; B, 0.94 ~1.1mas%; the balance is Fe; wherein, mas% refers to the mass percentage of the components in the main alloy raw material;所述辅合金原料包括以下组分:轻稀土元素LR,0~30.0mas%;LR为Nd和/或Pr;重稀土元素HR,1~80mas%;HR为Dy和/或Tb;M,5.0~20.0mas%;M选自Co、Cu、Al和Ga中的一种或多种;X,3.0~12.0mas%;X选自Ti、Zr、Hf、Nb、W和Ta中的一种或多种;B,0~0.6mas%;余量为Fe;其中,mas%是指组分在所述辅合金原料中的质量百分比;The auxiliary alloy raw material includes the following components: light rare earth element LR, 0-30.0 mas%; LR is Nd and/or Pr; heavy rare earth element HR, 1-80 mas%; HR is Dy and/or Tb; M, 5.0 ~20.0mas%; M is selected from one or more of Co, Cu, Al and Ga; X, 3.0~12.0mas%; X is selected from one or more of Ti, Zr, Hf, Nb, W and Ta Various; B, 0-0.6 mas%; the balance is Fe; wherein, mas% refers to the mass percentage of the components in the auxiliary alloy raw material;所述辅合金原料在所述主辅合金系钕铁硼磁体材料的原料组合物中的质量百分比为1.0~15.0mas%。The mass percentage of the auxiliary alloy raw material in the raw material composition of the main and auxiliary alloy-based NdFeB magnet material is 1.0-15.0 mas%.
- 如权利要求1所述的主辅合金系钕铁硼磁体材料的原料组合物,其特征在于,所述主合金原料中总稀土含量TRE为26.0~40.0mas%,较佳地为29.0~32.0mas%,例如29.5mas%、30.5mas%或31.5mas%,mas%是指组分在所述主合金原料中的质量百分比;The raw material composition of main and auxiliary alloy-based NdFeB magnet materials according to claim 1, wherein the total rare earth content TRE in the main alloy raw material is 26.0-40.0 mas%, preferably 29.0-32.0 mas %, such as 29.5mas%, 30.5mas% or 31.5mas%, mas% refers to the mass percentage of the components in the main alloy raw material;和/或,所述主合金原料中,所述LR的含量为25.0~30.0mas%,例如25.2mas%、29.5mas%或30mas%,mas%是指组分在所述主合金原料中的质量百分比;And/or, in the main alloy raw material, the content of the LR is 25.0-30.0 mas%, such as 25.2 mas%, 29.5 mas% or 30 mas%, and mas% refers to the mass of the components in the main alloy raw material percentage;和/或,所述主合金原料中,当所述LR包含Nd时,所述Nd的含量为18.9~22.5mas%,例如22.125mas%;当所述LR包含Pr时,所述Pr的含量为6.0~7.5mas%,例如6.3mas%或7.375mas%;其中,mas%是指组分在所述主合金原料中的质量百分比;And/or, in the main alloy raw material, when the LR contains Nd, the content of the Nd is 18.9-22.5 mas%, for example, 22.125 mas%; when the LR contains Pr, the content of the Pr is 6.0~7.5mas%, such as 6.3mas% or 7.375mas%; wherein, mas% refers to the mass percentage of the components in the main alloy raw material;和/或,所述主合金原料中,所述LR包含Nd和Pr;更佳地,所述Nd的含量为22.125mas%,所述Pr的含量为7.375mas%;或者,所述Nd的含 量为22.5mas%,所述Pr的含量为7.5mas%;或者,所述Nd的含量为18.9mas%,所述Pr的含量为6.3mas%;其中,mas%是指组分在所述主合金原料中的质量百分比;And/or, in the main alloy raw material, the LR contains Nd and Pr; more preferably, the content of the Nd is 22.125 mas%, and the content of the Pr is 7.375 mas%; or, the content of the Nd is 22.5mas%, and the Pr content is 7.5mas%; or, the Nd content is 18.9mas%, and the Pr content is 6.3mas%; wherein, mas% refers to the composition in the main alloy The mass percentage in the raw material;和/或,所述主合金原料中,所述HR的含量为1.0~10.0mas%,例如1.5mas%或5.3mas%,mas%是指组分在所述主合金原料中的质量百分比;And/or, in the main alloy raw material, the HR content is 1.0-10.0 mas%, for example, 1.5 mas% or 5.3 mas%, and mas% refers to the mass percentage of the components in the main alloy raw material;和/或,所述主合金原料中,当所述HR包含Dy时,所述Dy的含量为1.0~5.0mas%,例如1.5mas%或4.3mas%;较佳地,所述主合金原料中,所述HR为Dy;所述Dy的含量较佳地为1.5mas%;当所述HR包含Ho时,所述Ho的含量为0.5~2.0mas%,例如1.0mas%;其中,mas%是指组分在所述主合金原料中的质量百分比;And/or, in the main alloy raw material, when the HR contains Dy, the content of Dy is 1.0-5.0 mas%, such as 1.5 mas% or 4.3 mas%; preferably, in the main alloy raw material , the HR is Dy; the content of Dy is preferably 1.5mas%; when the HR contains Ho, the content of the Ho is 0.5-2.0mas%, for example 1.0mas%; wherein, mas% is Refers to the mass percentage of the components in the main alloy raw material;和/或,所述主合金原料中,所述HR包含Dy和Ho;其中,所述Dy的含量较佳地为4.3mas%,所述Ho的含量较佳地为1.0mas%,mas%是指组分在所述主合金原料中的质量百分比;And/or, in the main alloy raw material, the HR contains Dy and Ho; wherein, the content of the Dy is preferably 4.3 mas%, the content of the Ho is preferably 1.0 mas%, and the mas% is Refers to the mass percentage of the components in the main alloy raw material;和/或,所述主合金原料中,所述M的含量为0.5~2.0mas%,例如0.88mas%、1.5mas%或1.65mas%,mas%是指组分在所述主合金原料中的质量百分比;And/or, in the main alloy raw material, the content of M is 0.5-2.0 mas%, such as 0.88 mas%, 1.5 mas% or 1.65 mas%, where mas% refers to the percentage of the components in the main alloy raw material. mass percentage;和/或,所述主合金原料中,当所述M包含Ga时,所述Ga的含量为0.2~0.4mas%,例如0.25mas%;当所述M包含Al时,所述Al的含量为0.01~0.1mas%,例如0.03mas%;当所述M包含Cu时,所述Cu的含量为0.1~0.25mas%,例如0.15mas%;当所述M包含Co时,所述Co的含量为0.5~1.0mas%;其中,mas%是指组分在所述主合金原料中的质量百分比;And/or, in the main alloy raw material, when the M contains Ga, the content of the Ga is 0.2-0.4 mas%, for example, 0.25 mas%; when the M contains Al, the content of the Al is 0.01-0.1mas%, such as 0.03mas%; when the M includes Cu, the content of the Cu is 0.1-0.25mas%, such as 0.15mas%; when the M includes Co, the content of the Co is 0.5-1.0 mas%; wherein, mas% refers to the mass percentage of the components in the main alloy raw material;和/或,所述主合金原料中,所述M包含Ga、Al、Cu和Co;其中,所述Ga的含量较佳地为0.25mas%,所述Al的含量较佳地为0.03mas%,所述Cu的含量较佳地为0.1mas%,所述Co的含量较佳地为0.5mas%,mas%是指组分在所述主合金原料中的质量百分比;And/or, in the main alloy raw material, the M contains Ga, Al, Cu and Co; wherein, the content of the Ga is preferably 0.25mas%, and the content of the Al is preferably 0.03mas% , the content of Cu is preferably 0.1mas%, the content of Co is preferably 0.5mas%, and mas% refers to the mass percentage of the components in the main alloy raw material;和/或,所述主合金原料中,所述X的含量为0.1~0.35mas%,例如0.11mas%或0.15mas%,mas%是指组分在所述主合金原料中的质量百分比;And/or, in the main alloy raw material, the content of X is 0.1-0.35 mas%, for example, 0.11 mas% or 0.15 mas%, and mas% refers to the mass percentage of the components in the main alloy raw material;和/或,所述主合金原料中,所述X为Zr或Ti;And/or, in the main alloy raw material, the X is Zr or Ti;和/或,所述主合金原料中,所述B的含量为0.97~0.99mas%,例如0.98mas%,mas%是指组分在所述主合金原料中的质量百分比。And/or, in the main alloy raw material, the content of B is 0.97-0.99 mas%, for example, 0.98 mas%, and mas% refers to the mass percentage of the component in the main alloy raw material.
- 如权利要求1所述的主辅合金系钕铁硼磁体材料的原料组合物,其特征在于,所述主合金原料包括以下组分:Nd,22.125mas%;Pr,7.375mas%;Ga,0.25mas%;Al,0.03mas%;Cu,0.1mas%;Co,0.5mas%;Zr,0.11mas%;B,0.98mas%;余量为Fe;其中,mas%是指组分在所述主合金原料中的质量百分比;The raw material composition of main and auxiliary alloy-based NdFeB magnet materials according to claim 1, wherein the main alloy raw material comprises the following components: Nd, 22.125mas%; Pr, 7.375mas%; Ga, 0.25 mas%; Al, 0.03mas%; Cu, 0.1mas%; Co, 0.5mas%; Zr, 0.11mas%; B, 0.98mas%; The mass percentage in the alloy raw material;或者,所述主合金原料包括以下组分:Nd,22.5mas%;Pr,7.5mas%;Dy,1.5mas%;Ga,0.4mas%;Cu,0.25mas%;Co,1.0mas%;Zr,0.35mas%;B,0.97mas%;余量为Fe;其中,mas%是指组分在所述主合金原料中的质量百分比;Alternatively, the main alloy raw material includes the following components: Nd, 22.5mas%; Pr, 7.5mas%; Dy, 1.5mas%; Ga, 0.4mas%; Cu, 0.25mas%; Co, 1.0mas%; Zr, 0.35mas%; B, 0.97mas%; the balance is Fe; wherein, mas% refers to the mass percentage of components in the main alloy raw material;或者,所述主合金原料包括以下组分:Nd,18.9mas%;Pr,6.3mas%;Dy,4.3mas%;Ho,1.0mas%;Ga,0.25mas%;Al,0.1mas%;Cu,0.15mas%;Co,1.0mas%;Ti,0.15mas%;B,0.97mas%;余量为Fe;其中,mas%是指组分在所述主合金原料中的质量百分比。Alternatively, the main alloy raw material includes the following components: Nd, 18.9mas%; Pr, 6.3mas%; Dy, 4.3mas%; Ho, 1.0mas%; Ga, 0.25mas%; Al, 0.1mas%; Cu, 0.15mas%; Co, 1.0mas%; Ti, 0.15mas%; B, 0.97mas%; the balance is Fe; wherein, mas% refers to the mass percentage of components in the main alloy raw material.
- 如权利要求1所述的主辅合金系钕铁硼磁体材料的原料组合物,其特征在于,所述辅合金原料中总稀土含量TRE为35.0~50.0mas%,较佳地为40.0~45.0mas%,mas%是指组分在所述辅合金原料中的质量百分比;The raw material composition of main and auxiliary alloy-based NdFeB magnet materials according to claim 1, wherein the total rare earth content TRE in the auxiliary alloy raw material is 35.0-50.0 mas%, preferably 40.0-45.0 mas %, mas% refers to the mass percentage of the components in the auxiliary alloy raw material;和/或,所述辅合金原料中,所述LR的含量为20.0~30.0mas%,例如25.0mas%,mas%是指组分在所述辅合金原料中的质量百分比;And/or, in the auxiliary alloy raw material, the content of the LR is 20.0-30.0 mas%, for example, 25.0 mas%, and mas% refers to the mass percentage of the components in the auxiliary alloy raw material;和/或,所述辅合金原料中,当所述LR包含Nd时,所述Nd的含量为10.0~20.0mas%,例如15.0mas%;当所述LR包含Pr时,所述Pr的含量为15.0~25.0mas%,例如20.0mas%;其中,mas%是指组分在所述辅合金原料中的质量百分比;And/or, in the auxiliary alloy raw material, when the LR contains Nd, the content of the Nd is 10.0-20.0 mas%, for example, 15.0 mas%; when the LR contains Pr, the content of the Pr is 15.0~25.0mas%, for example 20.0mas%; wherein, mas% refers to the mass percentage of the components in the auxiliary alloy raw material;和/或,所述辅合金原料中,所述LR为Nd和Pr,所述Nd的含量为15.0mas%,所述Pr的含量为15.0mas%;mas%是指组分在所述辅合金原料 中的质量百分比;And/or, in the auxiliary alloy raw material, the LR is Nd and Pr, the content of Nd is 15.0 mas%, and the content of Pr is 15.0 mas%; mas% refers to the components in the auxiliary alloy. The mass percentage in the raw material;和/或,所述辅合金原料中,所述HR的含量为15.0~20.0mas%,mas%是指组分在所述辅合金原料中的质量百分比;And/or, in the auxiliary alloy raw material, the HR content is 15.0-20.0 mas%, and mas% refers to the mass percentage of the components in the auxiliary alloy raw material;和/或,所述辅合金原料中,所述HR为Tb,所述Tb的含量为15.0mas%,mas%是指组分在所述辅合金原料中的质量百分比;And/or, in the auxiliary alloy raw material, the HR is Tb, the content of the Tb is 15.0 mas%, and mas% refers to the mass percentage of the components in the auxiliary alloy raw material;和/或,所述辅合金原料中,所述HR为Dy,所述Dy的含量为20.0mas%,mas%是指组分在所述辅合金原料中的质量百分比;And/or, in the auxiliary alloy raw material, the HR is Dy, the content of the Dy is 20.0 mas%, and mas% refers to the mass percentage of the components in the auxiliary alloy raw material;和/或,所述辅合金原料中,当所述M包含Ga时,所述Ga的含量为2.0~10.0mas%,例如5.0mas%;当所述M包含Co时,所述Co的含量为10.0~20.0mas%,例如15.0mas%;其中,mas%是指组分在所述辅合金原料中的质量百分比;And/or, in the auxiliary alloy raw material, when the M contains Ga, the content of the Ga is 2.0-10.0 mas%, for example, 5.0 mas%; when the M contains Co, the content of the Co is 10.0-20.0mas%, for example 15.0mas%; wherein, mas% refers to the mass percentage of the components in the auxiliary alloy raw material;和/或,所述辅合金原料中,所述M为Ga和Co;其中,所述Ga的含量较佳地为5.0mas%,所述Co的含量较佳地为15.0mas%,mas%是指组分在所述辅合金原料中的质量百分比;And/or, in the auxiliary alloy raw material, the M is Ga and Co; wherein, the content of the Ga is preferably 5.0mas%, the content of the Co is preferably 15.0mas%, and the mas% is Refers to the mass percentage of the components in the auxiliary alloy raw material;和/或,所述辅合金原料中,所述X的含量为4.0~10.0mas%,例如4.5mas%或5.0mas%,mas%是指组分在所述辅合金原料中的质量百分比;较佳地,所述辅合金原料中,所述X为Zr;And/or, in the auxiliary alloy raw material, the content of X is 4.0-10.0 mas%, for example, 4.5 mas% or 5.0 mas%, and mas% refers to the mass percentage of the components in the auxiliary alloy raw material; Preferably, in the auxiliary alloy raw material, the X is Zr;和/或,所述辅合金原料中,所述B的含量为0.3~0.6mas%,例如0.4mas%或0.5mas%,mas%是指组分在所述辅合金原料中的质量百分比;And/or, in the auxiliary alloy raw material, the content of B is 0.3-0.6 mas%, for example, 0.4 mas% or 0.5 mas%, and mas% refers to the mass percentage of the component in the auxiliary alloy raw material;和/或,所述辅合金原料在所述主辅合金系钕铁硼磁体材料的原料组合物中的质量百分比为2.0~5.0mas%,例如4.0mas%。And/or, the mass percentage of the auxiliary alloy raw material in the raw material composition of the main and auxiliary alloy-based NdFeB magnet material is 2.0-5.0 mas%, for example, 4.0 mas%.
- 如权利要求1所述的主辅合金系钕铁硼磁体材料的原料组合物,其特征在于,所述辅合金原料包括以下组分:Nd,15.0mas%;Pr,15.0mas%;Tb,15.0mas%;Zr,10.0mas%;B,0.5mas%;余量为Fe;其中,mas%是指组分在所述辅合金原料中的质量百分比;The raw material composition of main and auxiliary alloy-based NdFeB magnet materials according to claim 1, wherein the auxiliary alloy raw material comprises the following components: Nd, 15.0mas%; Pr, 15.0mas%; Tb, 15.0 mas%; Zr, 10.0mas%; B, 0.5mas%; the balance is Fe; wherein, mas% refers to the mass percentage of components in the auxiliary alloy raw material;或者,所述辅合金原料包括以下组分:Pr,25.0mas%;Dy,20.0mas%;Zr,4.5mas%;B,0.5mas%;余量为Fe;其中,mas%是指组分在所述辅合 金原料中的质量百分比;Alternatively, the auxiliary alloy raw material includes the following components: Pr, 25.0mas%; Dy, 20.0mas%; Zr, 4.5mas%; B, 0.5mas%; The mass percentage in the auxiliary alloy raw material;或者,所述辅合金原料包括以下组分:Pr,20.0mas%;Dy,20.0mas%;Ga,5.0mas%;Co,15.0mas%;Zr,5.0mas%;B,0.4mas%;余量为Fe;其中,mas%是指组分在所述辅合金原料中的质量百分比。Alternatively, the auxiliary alloy raw material includes the following components: Pr, 20.0mas%; Dy, 20.0mas%; Ga, 5.0mas%; Co, 15.0mas%; Zr, 5.0mas%; B, 0.4mas%; balance is Fe; wherein, mas% refers to the mass percentage of the components in the auxiliary alloy raw material.
- 如权利要求1所述的主辅合金系钕铁硼磁体材料的原料组合物,其特征在于,所述主辅合金系钕铁硼磁体材料的原料组合物包括主合金原料和辅合金原料;其中,所述主合金原料包括以下组分:Nd,22.125mas%;Pr,7.375mas%;Ga,0.25mas%;Al,0.03mas%;Cu,0.1mas%;Co,0.5mas%;Zr,0.11mas%;B,0.98mas%;余量为Fe;其中,mas%是指组分在所述主合金原料中的质量百分比;所述辅合金原料包括以下组分:Nd,15.0mas%;Pr,15.0mas%;Tb,15.0mas%;Zr,10.0mas%;B,0.5mas%;余量为Fe;其中,mas%是指组分在所述辅合金原料中的质量百分比;所述辅合金原料在所述主辅合金系钕铁硼磁体材料的原料组合物中的质量百分比为4.0mas%;The raw material composition of the main and auxiliary alloy-based NdFeB magnet materials according to claim 1, wherein the raw material composition of the main and auxiliary alloy-based NdFeB magnet materials comprises a main alloy raw material and an auxiliary alloy raw material; wherein , the main alloy raw material includes the following components: Nd, 22.125mas%; Pr, 7.375mas%; Ga, 0.25mas%; Al, 0.03mas%; Cu, 0.1mas%; Co, 0.5mas%; Zr, 0.11 mas%; B, 0.98mas%; the balance is Fe; wherein, mas% refers to the mass percentage of components in the main alloy raw material; the auxiliary alloy raw material includes the following components: Nd, 15.0mas%; Pr , 15.0mas%; Tb, 15.0mas%; Zr, 10.0mas%; B, 0.5mas%; the balance is Fe; The mass percentage of alloy raw materials in the raw material composition of the main and auxiliary alloy-based NdFeB magnet materials is 4.0 mas%;或者,所述主辅合金系钕铁硼磁体材料的原料组合物包括主合金原料和辅合金原料;其中,所述主合金原料包括以下组分:Nd,22.5mas%;Pr,7.5mas%;Dy,1.5mas%;Ga,0.4mas%;Cu,0.25mas%;Co,1.0mas%;Zr,0.35mas%;B,0.97mas%;余量为Fe;其中,mas%是指组分在所述主合金原料中的质量百分比;所述辅合金原料包括以下组分:Pr,25.0mas%;Dy,20.0mas%;Zr,4.5mas%;B,0.5mas%;余量为Fe;其中,mas%是指组分在所述辅合金原料中的质量百分比;所述辅合金原料在所述主辅合金系钕铁硼磁体材料的原料组合物中的质量百分比为5.0mas%;Alternatively, the raw material composition of the main and auxiliary alloy-based NdFeB magnet materials includes a main alloy raw material and an auxiliary alloy raw material; wherein, the main alloy raw material includes the following components: Nd, 22.5mas%; Pr, 7.5mas%; Dy, 1.5mas%; Ga, 0.4mas%; Cu, 0.25mas%; Co, 1.0mas%; Zr, 0.35mas%; B, 0.97mas%; The mass percentage in the main alloy raw material; the auxiliary alloy raw material includes the following components: Pr, 25.0mas%; Dy, 20.0mas%; Zr, 4.5mas%; B, 0.5mas%; the balance is Fe; wherein , mas% refers to the mass percentage of the components in the auxiliary alloy raw materials; the mass percentage of the auxiliary alloy raw materials in the raw material composition of the main and auxiliary alloy NdFeB magnet materials is 5.0 mas%;或者,所述主辅合金系钕铁硼磁体材料的原料组合物包括主合金原料和辅合金原料;其中,所述主合金原料包括以下组分:Nd,18.9mas%;Pr,6.3mas%;Dy,4.3mas%;Ho,1.0mas%;Ga,0.25mas%;Al,0.1mas%;Cu,0.15mas%;Co,1.0mas%;Zr,0.2mas%;B,0.97mas%;余量为Fe;其中,mas%是指组分在所述主合金原料中的质量百分比;所述辅合金原料 包括以下组分:Pr,20.0mas%;Dy,20.0mas%;Ga,5.0mas%;Co,15.0mas%;Zr,5.0mas%;B,0.4mas%;余量为Fe;其中,mas%是指组分在所述辅合金原料中的质量百分比;所述辅合金原料在所述主辅合金系钕铁硼磁体材料的原料组合物中的质量百分比为4.0mas%。Alternatively, the raw material composition of the main and auxiliary alloy-based NdFeB magnet materials includes a main alloy raw material and an auxiliary alloy raw material; wherein, the main alloy raw material includes the following components: Nd, 18.9 mas%; Pr, 6.3 mas%; Dy, 4.3mas%; Ho, 1.0mas%; Ga, 0.25mas%; Al, 0.1mas%; Cu, 0.15mas%; Co, 1.0mas%; Zr, 0.2mas%; B, 0.97mas%; is Fe; wherein, mas% refers to the mass percentage of components in the main alloy raw material; the auxiliary alloy raw material includes the following components: Pr, 20.0mas%; Dy, 20.0mas%; Ga, 5.0mas%; Co, 15.0mas%; Zr, 5.0mas%; B, 0.4mas%; the balance is Fe; wherein, mas% refers to the mass percentage of the components in the auxiliary alloy raw material; The mass percentage in the raw material composition of the main and auxiliary alloy-based NdFeB magnet material is 4.0 mas%.
- 一种主辅合金系钕铁硼磁体材料的制备方法,其包括以下步骤:A preparation method of a main and auxiliary alloy system NdFeB magnet material, which comprises the following steps:S1、将如权利要求1~6中任一项所述的主辅合金系钕铁硼磁体材料的原料组合物中的所述主合金原料和所述辅合金原料分别熔融后铸造,分别得主合金和辅合金;S1. The main alloy raw material and the auxiliary alloy raw material in the raw material composition of the main and auxiliary alloy-based NdFeB magnet materials according to any one of claims 1 to 6 are respectively melted and then casted to obtain the main alloy. and auxiliary alloys;S2、将所述主合金和所述辅合金分别氢破碎和微粉碎后混合,进行成型和烧结处理,即得所述主辅合金系钕铁硼磁体材料。S2. The main alloy and the auxiliary alloy are hydrogen crushed and finely pulverized, respectively, and then mixed, and subjected to forming and sintering treatment to obtain the main and auxiliary alloy NdFeB magnet material.
- 如权利要求7所述的主辅合金系钕铁硼磁体材料的制备方法,其特征在于,所述熔融在熔炼炉中熔炼,所述熔炼炉的真空度约为5×10 -2Pa,所述熔炼的温度为1300℃~1600℃,较佳地为1500℃~1550℃; The method for preparing main and auxiliary alloy NdFeB magnet materials according to claim 7, wherein the melting is performed in a smelting furnace, and the vacuum degree of the smelting furnace is about 5×10 -2 Pa, so The smelting temperature is 1300℃~1600℃, preferably 1500℃~1550℃;和/或,所述铸造的工艺为薄带连铸法、铸锭法、离心铸造法或快淬法;And/or, the casting process is thin strip continuous casting, ingot casting, centrifugal casting or rapid quenching;和/或,所述氢破碎的脱氢温度为400℃~650℃,例如500~620℃;And/or, the dehydrogenation temperature of the hydrogen fragmentation is 400 to 650°C, for example, 500 to 620°C;和/或,所述微粉碎在气流磨中进行;and/or, the micro-grinding is carried out in a jet mill;和/或,所述微粉碎在含氧气氛下进行;所述含氧气氛中氧含量较佳地为80ppm以下,更佳地为50ppm以下;And/or, the micro-pulverization is carried out in an oxygen-containing atmosphere; the oxygen content in the oxygen-containing atmosphere is preferably below 80 ppm, more preferably below 50 ppm;和/或,所述微粉碎后的粉末粒径为1~20μm;And/or, the particle size of the finely pulverized powder is 1-20 μm;和/或,所述成型为在压机中压制成为生坯;所述压机的磁场强度较佳地为0.5T~3.0T,例如1.0~2.0T;所述压制的压力较佳地为200~300MPa,例如260MPa;所述压制的时间较佳地为3~30s,例如15s;And/or, the forming is to press in a press to form a green body; the magnetic field strength of the press is preferably 0.5T to 3.0T, for example, 1.0 to 2.0T; the pressing pressure is preferably 200 ~300MPa, such as 260MPa; the pressing time is preferably 3-30s, such as 15s;和/或,所述烧结的温度为1000℃~1150℃,较佳地为1060~1090℃;And/or, the temperature of the sintering is 1000-1150°C, preferably 1060-1090°C;和/或,所述烧结的时间为4~20小时;And/or, the sintering time is 4-20 hours;和/或,所述烧结的气氛为真空或氩气气氛。And/or, the sintering atmosphere is vacuum or argon atmosphere.
- 一种主辅合金系钕铁硼磁体材料,其根据权利要求7或8所述的主辅合金系钕铁硼磁体材料的制备方法制备得到。A main and auxiliary alloy system NdFeB magnet material is prepared according to the preparation method of the main and auxiliary alloy system NdFeB magnet material according to claim 7 or 8.
- 如权利要求9所述的主辅合金系钕铁硼磁体材料,其特征在于,所述主辅合金系钕铁硼磁体材料包括主相和晶界相;其中,所述主相为核壳结构,所述核为LR 2T 14B,所述壳为HR 2T 14B;所述晶界相包括富钕相、XB 2相和R 6T 13M相;其中,R为LR和/或HR;LR选自Y、La、Ce、Pr、Nd的一种或多种;HR选自Gd、Dy、Tb和Ho中的一种或多种;M选自Cu、Al和Ga中的一种或多种;X选自Ti、Zr、Hf、Nb、W和Ta中的一种或多种;T为Fe和/或Co; The main and auxiliary alloy NdFeB magnet material according to claim 9, wherein the main and auxiliary alloy NdFeB magnet material comprises a main phase and a grain boundary phase; wherein, the main phase is a core-shell structure , the core is LR 2 T 14 B, and the shell is HR 2 T 14 B; the grain boundary phase includes neodymium-rich phase, XB 2 phase and R 6 T 13 M phase; wherein, R is LR and/or HR; LR is selected from one or more of Y, La, Ce, Pr, Nd; HR is selected from one or more of Gd, Dy, Tb and Ho; M is selected from one or more of Cu, Al and Ga one or more; X is selected from one or more of Ti, Zr, Hf, Nb, W and Ta; T is Fe and/or Co;较佳地,所述主辅合金系钕铁硼磁体材料中,LR为Pr和Nd;HR为Tb;M为Cu、Al和Ga;X为Zr;T为Fe和Co;Preferably, in the main and auxiliary alloy NdFeB magnet materials, LR is Pr and Nd; HR is Tb; M is Cu, Al and Ga; X is Zr; T is Fe and Co;较佳地,所述主辅合金系钕铁硼磁体材料中,LR为Pr和Nd;HR为Dy;M为Cu和Ga;X为Zr;T为Fe和Co;Preferably, in the main and auxiliary alloy NdFeB magnet materials, LR is Pr and Nd; HR is Dy; M is Cu and Ga; X is Zr; T is Fe and Co;较佳地,所述主辅合金系钕铁硼磁体材料中,LR为Pr和Nd;HR为Dy和Ho;M为Cu、Al和Ga;X为Ti;T为Fe和Co。Preferably, in the main and auxiliary alloy NdFeB magnet materials, LR is Pr and Nd; HR is Dy and Ho; M is Cu, Al and Ga; X is Ti; T is Fe and Co.
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WO2011122667A1 (en) * | 2010-03-30 | 2011-10-06 | Tdk株式会社 | Rare earth sintered magnet, method for producing the same, motor, and automobile |
CN103103442A (en) * | 2013-02-28 | 2013-05-15 | 包头稀土研究院 | Method for preparing neodymium-iron-boron material through main-auxiliary alloy method |
CN103617855A (en) * | 2013-11-30 | 2014-03-05 | 宁波科星材料科技有限公司 | Neodymium iron boron magnetic material with excellent magnetic performance |
CN108389711A (en) * | 2018-01-05 | 2018-08-10 | 宁波招宝磁业有限公司 | A kind of preparation method of the Sintered NdFeB magnet with high-coercive force |
CN111613403A (en) * | 2020-06-01 | 2020-09-01 | 福建省长汀金龙稀土有限公司 | Neodymium-iron-boron magnet material, raw material composition, preparation method and application thereof |
-
2021
- 2021-03-10 CN CN202110261268.0A patent/CN115083707A/en active Pending
-
2022
- 2022-01-17 EP EP22766077.6A patent/EP4307325A1/en active Pending
- 2022-01-17 KR KR1020237025822A patent/KR20230126733A/en unknown
- 2022-01-17 JP JP2023544205A patent/JP2024512183A/en active Pending
- 2022-01-17 WO PCT/CN2022/072244 patent/WO2022188550A1/en active Application Filing
- 2022-02-25 TW TW111107190A patent/TW202235640A/en unknown
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011122667A1 (en) * | 2010-03-30 | 2011-10-06 | Tdk株式会社 | Rare earth sintered magnet, method for producing the same, motor, and automobile |
CN103103442A (en) * | 2013-02-28 | 2013-05-15 | 包头稀土研究院 | Method for preparing neodymium-iron-boron material through main-auxiliary alloy method |
CN103617855A (en) * | 2013-11-30 | 2014-03-05 | 宁波科星材料科技有限公司 | Neodymium iron boron magnetic material with excellent magnetic performance |
CN108389711A (en) * | 2018-01-05 | 2018-08-10 | 宁波招宝磁业有限公司 | A kind of preparation method of the Sintered NdFeB magnet with high-coercive force |
CN111613403A (en) * | 2020-06-01 | 2020-09-01 | 福建省长汀金龙稀土有限公司 | Neodymium-iron-boron magnet material, raw material composition, preparation method and application thereof |
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EP4307325A1 (en) | 2024-01-17 |
KR20230126733A (en) | 2023-08-30 |
CN115083707A (en) | 2022-09-20 |
JP2024512183A (en) | 2024-03-19 |
TW202235640A (en) | 2022-09-16 |
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